CN111073467A - Corrosion-resistant composite protective layer material for neodymium iron boron - Google Patents
Corrosion-resistant composite protective layer material for neodymium iron boron Download PDFInfo
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- C09D5/18—Fireproof paints including high temperature resistant paints
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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Abstract
The invention discloses a corrosion-resistant composite protective layer material for neodymium iron boron, which comprises the following components in parts by weight: the base layer is coated on the neodymium iron boron in a spinning mode; the protective layer is coated on the substrate layer; the protective layer is composed of the following raw materials in parts by weight: 10-20 parts of fluorine-containing methacrylate, 30-50 parts of epoxy resin, 40-60 parts of vinyl epoxy resin, 5-10 parts of additive, 0.5-1.5 parts of curing agent, 1-2.5 parts of filler and 20-50 parts of deionized water. According to the composite protective layer material, the double-layer structure of the substrate layer and the protective layer is arranged, so that the surface corrosion resistance of the neodymium iron boron permanent magnet can be improved, the wear resistance and the heat resistance of the neodymium iron boron permanent magnet can be improved, and the service life of the neodymium iron boron surface protective layer is prolonged.
Description
Technical Field
The invention relates to the technical field of neodymium iron boron, in particular to a corrosion-resistant composite protective layer material for neodymium iron boron.
Background
The neodymium iron boron is divided into sintered neodymium iron boron and bonded neodymium iron boron, and the bonded neodymium iron boron is magnetic in all directions and is corrosion-resistant; the sintered neodymium iron boron is easy to corrode, and the surface of the sintered neodymium iron boron needs to be plated with zinc, nickel, environment-friendly zinc, environment-friendly nickel, nickel copper nickel, environment-friendly nickel copper nickel and the like. Compared with the traditional permanent magnet material, the sintered Nd-Fe-B permanent magnet has excellent characteristics and cost performance, and is widely applied to various industries such as computers, motors, electric vehicles, instruments and meters, magnetic transmission bearings, high-fidelity speakers, nuclear magnetic resonance imaging instruments, aerospace and aviation and the like. China vigorously develops the industry of the neodymium iron boron magnet by virtue of the advantages of rare earth resources and production cost, and has become the first producing and consuming countries in the world.
In general, the basic approach to improve the corrosion resistance of materials can be considered from the aspects of improving the corrosion resistance of the materials and protecting the surfaces of the materials from coating. The protection of the surface of the material can be realized by methods such as electroplating, chemical plating, organic coating, physical vapor deposition and the like. The organic coating has the problems of weak binding force between the organic polymer coating and the neodymium iron boron substrate, great environmental pollution in the surface treatment process, poor wear resistance and weather resistance of the coating and the like.
Therefore, a coating with good environmental protection, wear resistance, corrosion resistance and weather resistance is yet to be developed.
Disclosure of Invention
In view of the defects of the prior art, the invention provides a corrosion-resistant composite protective layer material for neodymium iron boron, which meets the requirement of high corrosion resistance of a neodymium iron boron surface protective layer, and enables the neodymium iron boron surface protective layer to have good heat resistance, wear resistance and weather resistance so as to prolong the service life of a neodymium iron boron magnet.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
a corrosion resistant composite armor material for neodymium iron boron, the composite armor material comprising:
the base layer is coated on the neodymium iron boron in a spinning mode; and
the protective layer is coated on the substrate layer;
the protective layer is composed of the following raw materials in parts by weight: 10-20 parts of fluorine-containing methacrylate, 30-50 parts of epoxy resin, 40-60 parts of vinyl epoxy resin, 5-10 parts of additive, 0.5-1.5 parts of curing agent, 1-2.5 parts of filler and 20-50 parts of deionized water.
According to the protective layer, epoxy resin and vinyl epoxy resin are used as main raw materials for polymerization reaction, fluorine-containing methacrylate is added to carry out copolymerization reaction with the main raw materials, so that the epoxy resin organic protective layer is subjected to modification treatment, and the fluorine-containing group has a hydrophobic effect on the one hand, so that water stains on the surface of neodymium iron boron are prevented from permeating into the neodymium iron boron matrix, and the oxidation effect of the neodymium iron boron is intensified; on the other hand, the fluorine-containing group also improves the weather resistance of the neodymium iron boron surface protective layer.
The base layer is composed of the following raw materials in parts by weight: 30-60 parts of epoxy resin, 10-30 parts of hydroxyl epoxy resin, 1-5 parts of additive, 1-3 parts of triisocyanate compound, 0.5-1.5 parts of hexamethylene diisocyanate, 0.05-0.15 part of organic tin catalyst, 0.1-1 part of nano titanium dioxide and 20-50 parts of deionized water.
According to the base layer, the epoxy resin and the hydroxyl epoxy resin are used as main raw materials for the polymerization reaction of the base layer, the triisocyanate compound and the hexamethylene diisocyanate are added, the bonding strength between the base layer and the neodymium iron boron substrate is further enhanced, in addition, the triisocyanate compound and the hydroxyl functional group in the main raw materials are subjected to a grafting reaction under the action of an organic tin catalyst, in the reaction process, the triisocyanate compound forms a ring structure with stability, and the ageing resistance and the weather resistance of the base layer are improved. In the stratum basale, the nanometer titanium dioxide of adulteration can play the passageway of corrosive electrolyte liquid to the inside infiltration of stratum basale in the extension environment, increases the effect of stratum basale at neodymium iron boron base member edge thickness homogeneity, and then improves the life-span of in service of neodymium iron boron surface composite protection layer.
The additive is calix [4] arene.
The structural formula of the calix [4] arene is shown as a structural formula 1:
structural formula 1
In the structural formula 1, R1 and R2 are independently selected from H or C1-5 alkyl;
in the structural formula 1, in the formula,
expressed as a terminal olefin with a long chain structure that reduces steric hindrance upon free radical polymerization.
According to the invention, calix [4] arene shown as a structural formula 1 is selected as an additive and added into the base layer and the protective layer of the composite coating, so that the leveling and compatibility effects are effectively achieved, each obtained coating is more uniform, and the bonding property between the layers is stronger; the invention also effectively utilizes the unique inclusion characteristic of the calixarene structure, so that the filler is uniformly dispersed in the protective layer, thereby increasing the wear resistance of the surface of the neodymium iron boron matrix.
The calix [4] arene of the structural formula 1 is based on hydroxyl of tert-butyl calixarene, and under the catalytic action of ethylamine and titanium tetrachloride, the calix [4] arene of terminal olefin with a long-chain structure modified at the upper edge is obtained.
The fluorine-containing methacrylate is one or more of perfluorocyclohexyl methacrylate, pentafluorobenzyl methacrylate and 2,3,5, 6-tetrafluorophenyl methacrylate.
The curing agent is one or more of benzoyl peroxide, cumene hydroperoxide, tert-butyl hydroperoxide, 2, 4-dichlorobenzoyl peroxide and lauroyl peroxide.
The triisocyanate compound is one or more of 4,4',4' ' -triphenylmethane triisocyanate, undecane-1, 6, 11-triyl triisocyanate and toluene-2, 4, 6-triyl triisocyanate.
The organic tin catalyst is one or more of dibutyltin dilaurate, dibutyltin monomaleate and dibutyltin di (isooctylmercaptoacetate).
The filler is one or more of attapulgite powder, sepiolite powder, montmorillonite and mica powder.
The thickness of the base layer is 1 to 5 μm.
The thickness of the protective layer is 5-20 μm.
The preparation method of the substrate layer comprises the following steps: weighing the raw materials in parts by weight, placing 30-60 parts of epoxy resin, 10-30 parts of hydroxyl epoxy resin, 0.5-3.5 parts of additive, 1-3 parts of triisocyanate compound, 0.5-1.5 parts of hexamethylene diisocyanate, 0.1-1 part of nano titanium dioxide and 20-50 parts of deionized water in a stirring tank for uniform stirring, then adding 0.05-0.15 part of organic tin catalyst and 0.5-1.5 parts of additive, continuously stirring uniformly, spin-coating the uniformly stirred substrate layer mixed liquid on a neodymium iron boron substrate, and curing to obtain the neodymium iron boron with the surface coated with the substrate layer.
The preparation method of the protective layer comprises the following steps: weighing the raw materials in parts by weight, placing 10-20 parts of fluorine-containing methacrylate, 30-50 parts of epoxy resin, 40-60 parts of vinyl epoxy resin, 1-2.5 parts of filler, 3.5-7 parts of additive and 20-50 parts of deionized water in a stirring tank, uniformly stirring, adding 1.5-3 parts of additive and 0.5-1.5 parts of curing agent, continuously stirring uniformly, spin-coating the uniformly stirred protective layer mixed solution on a substrate layer, heating and curing to obtain the neodymium iron boron with the surface coated with the corrosion-resistant composite protective layer material.
The invention has the beneficial effects that:
the corrosion-resistant composite protective layer material for the neodymium iron boron is environment-friendly in formula, mainly comprises the water-based coating material, and the obtained substrate layer is strong in binding property with the neodymium iron boron substrate and has excellent oxidation resistance and weather resistance; the protective layer has excellent hydrophobicity, weather resistance and wear resistance; in general, through the structural design of the composite protective layer, the surface corrosion resistance of the neodymium iron boron permanent magnet is improved, and the service life of the neodymium iron boron surface protective layer is prolonged.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
Example 1
This embodiment is used for corrosion-resistant composite protective layer material of neodymium iron boron, and it includes:
the base layer is coated on the neodymium iron boron in a spinning mode; and
the protective layer is coated on the substrate layer;
the protective layer is composed of the following raw materials in parts by weight: 15 parts of fluorine-containing methacrylate, 40 parts of epoxy resin, 50 parts of vinyl epoxy resin, 7 parts of additive, 1 part of curing agent, 1.5 parts of filler and 30 parts of deionized water.
The base layer is composed of the following raw materials in parts by weight: 45 parts of epoxy resin, 20 parts of hydroxy epoxy resin, 3 parts of additive, 2 parts of triisocyanate compound, 1 part of hexamethylene diisocyanate, 0.1 part of organic tin catalyst, 0.5 part of nano titanium dioxide and 35 parts of deionized water.
The additive is calix [4] arene.
The structural formula of the calix [4] arene is shown as a structural formula 1:
structural formula 1
In the structural formula 1, R1 and R2 are respectively selected from H and C3 hydrocarbyl;
in the structural formula 1, in the formula,
as the terminal olefin having a long chain structure, preferred are pentenyl, octenyl, decenyl and isomers thereof, and more preferred is octenyl.
The fluorine-containing methacrylate is perfluorocyclohexyl methacrylate.
The curing agent is benzoyl peroxide.
The triisocyanate compound is 4,4',4' ' -triphenylmethane triisocyanate.
The organic tin catalyst is dibutyltin dilaurate.
The filler is attapulgite powder, and the mesh number of the filler is 1000 meshes.
The film thickness of the base layer is 3 μm.
The film thickness of the protective layer is 15 mu m.
Example 2
This embodiment is used for corrosion-resistant composite protective layer material of neodymium iron boron, and it includes:
the base layer is coated on the neodymium iron boron in a spinning mode; and
the protective layer is coated on the substrate layer;
the protective layer is composed of the following raw materials in parts by weight: 10 parts of fluorine-containing methacrylate, 30 parts of epoxy resin, 40 parts of vinyl epoxy resin, 5 parts of additive, 0.5 part of curing agent, 1 part of filler and 20 parts of deionized water.
The base layer is composed of the following raw materials in parts by weight: 30 parts of epoxy resin, 10 parts of hydroxyl epoxy resin, 1 part of additive, 1 part of triisocyanate compound, 0.5 part of hexamethylene diisocyanate, 0.05 part of organic tin catalyst, 0.1 part of nano titanium dioxide and 20 parts of deionized water.
The additive is calix [4] arene.
The structural formula of the calix [4] arene is shown as a structural formula 1:
structural formula 1
In the structural formula 1, R1 and R2 are respectively selected from H and C1 hydrocarbyl; (ii) a
In the structural formula 1, in the formula,
expressed as terminal olefins with long chain structures. Preferred are pentenyl, octenyl, decenyl and isomers thereof, and more preferred is octenyl.
The fluorine-containing methacrylate is pentafluorobenzyl methacrylate.
The curing agent is cumene hydroperoxide.
The triisocyanate compound is undecane-1, 6, 11-triyl triisocyanate.
The organic tin catalyst is monobutyl maleate dibutyltin.
The filler is montmorillonite, and the mesh number of the filler is 1500 meshes.
The film thickness of the base layer is 1 μm.
The film thickness of the protective layer is 5 mu m.
Example 3
This embodiment is used for corrosion-resistant composite protective layer material of neodymium iron boron, and it includes:
the base layer is coated on the neodymium iron boron in a spinning mode; and
the protective layer is coated on the substrate layer;
the protective layer is composed of the following raw materials in parts by weight: 20 parts of fluorine-containing methacrylate, 50 parts of epoxy resin, 60 parts of vinyl epoxy resin, 10 parts of additive, 1.5 parts of curing agent, 2.5 parts of filler and 50 parts of deionized water.
The base layer is composed of the following raw materials in parts by weight: 60 parts of epoxy resin, 30 parts of hydroxyl epoxy resin, 5 parts of additive, 3 parts of triisocyanate compound, 1.5 parts of hexamethylene diisocyanate, 0.15 part of organic tin catalyst, 1 part of nano titanium dioxide and 50 parts of deionized water.
The additive is calix [4] arene.
The structural formula of the calix [4] arene is shown as a structural formula 1:
structural formula 1
In the structural formula 1, R1 and R2 are respectively selected from H and C5 hydrocarbyl;
in the structural formula 1, in the formula,
expressed as terminal olefins with long chain structures. Preferred are pentenyl, octenyl, decenyl and isomers thereof, and more preferred is octenyl.
The fluorine-containing methacrylate is 2,3,5, 6-tetrafluorophenyl methacrylate.
The curing agent is tert-butyl hydroperoxide.
The triisocyanate compound is toluene-2, 4, 6-triyl triisocyanate.
The organic tin catalyst is dibutyltin di (isooctyl thioglycolate).
The filler is mica powder, and the mesh number of the filler is 1200 meshes.
The film thickness of the base layer is 5 μm.
The film thickness of the protective layer is 20 mu m.
Comparative example 1
The corrosion resistant composite armor material for ndfeb of this comparative example is substantially similar to example 1, with the primary difference being that the base layer does not contain additives.
Comparative example 2
The corrosion-resistant composite armor material for ndfeb of this comparative example is substantially similar to example 1, with the primary difference being that the armor does not contain additives.
Comparative example 3
The corrosion resistant composite armor material for neodymium iron boron of this comparative example is substantially similar to example 1 with the primary difference being that the armor does not include a fluoro-methacrylate.
The composite protective layer materials prepared in the examples 1-3 and the comparative examples 1-3 are subjected to performance tests, and the performance results are shown in the following table 1:
and (3) corrosion resistance testing: testing the salt spray corrosion resistance of a sample by using an SH-90 type salt spray corrosion test box according to GB/T2423.17-1993; the test environment temperature is (35 +/-2) DEG C, the pressure range is 0.8-1.2 Pa, the time of occurrence of corrosion is taken as the evaluation standard of the corrosion resistance of the neodymium iron boron, and the time is measured in hours.
And (3) weather resistance test: and (3) carrying out a salt spray test for 72h at the temperature of 120 ℃, and observing the appearance of the surface protective functional layer of the neodymium iron boron permanent magnet so as to judge the weather resistance of the neodymium iron boron permanent magnet.
And (3) testing heat resistance: the neodymium iron boron materials prepared by the preparation methods of the embodiments 1-3 and the comparative examples 1-3 are immersed in hot water at 80 ℃, heated for 24 hours, and the appearance of the surface protection function layer of the neodymium iron boron permanent magnet is observed to judge the heat resistance of the neodymium iron boron permanent magnet.
TABLE 1
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Corrosion resistance h | 476 | 441 | 489 | 413 | 388 | 423 |
| Weather resistance | Has no obvious defect | Has no obvious defect | Has no obvious defect | Local occurrence of exfoliation | Has no obvious defect | Large area of peeling |
| Wear resistance | Good effect | Good effect | Good effect | Good effect | Good effect | Good effect |
| Heat resistance | Has no obvious defect | Has no obvious defect | Has no obvious defect | Large area of peeling | Large area of peeling | Local occurrence of exfoliation |
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed.
Claims (10)
1. A corrosion resistant composite armor material for NdFeB, comprising:
the base layer is coated on the neodymium iron boron in a spinning mode; and
the protective layer is coated on the substrate layer;
the protective layer is composed of the following raw materials in parts by weight: 10-20 parts of fluorine-containing methacrylate, 30-50 parts of epoxy resin, 40-60 parts of vinyl epoxy resin, 5-10 parts of additive, 0.5-1.5 parts of curing agent, 1-2.5 parts of filler and 20-50 parts of deionized water.
2. The corrosion-resistant composite protective layer material for neodymium iron boron according to claim 1, wherein the base layer is composed of the following raw materials in parts by weight: 30-60 parts of epoxy resin, 10-30 parts of hydroxyl epoxy resin, 1-5 parts of additive, 1-3 parts of triisocyanate compound, 0.5-1.5 parts of hexamethylene diisocyanate, 0.05-0.15 part of organic tin catalyst, 0.1-1 part of nano titanium dioxide and 20-50 parts of deionized water.
3. The corrosion resistant composite armor material for neodymium iron boron according to claims 1 or 2, wherein said additive is calix [4] arene.
4. The corrosion resistant composite armor material for ndfeb according to claim 3, wherein the calix [4] arene has the structural formula shown in formula 1:
structural formula 1
In the structural formula 1, R1 and R2 are independently selected from H or C1～5A hydrocarbon group of (a);
in the structural formula 1, in the formula,
expressed as terminal olefins with long chain structures.
5. The corrosion resistant composite armor material for neodymium iron boron according to claim 1, wherein said fluorine-containing methacrylate is one or more of perfluorocyclohexyl methacrylate, pentafluorobenzyl methacrylate, 2,3,5, 6-tetrafluorophenyl methacrylate.
6. The corrosion-resistant composite protective layer material for neodymium iron boron according to claim 1, wherein the curing agent is selected from one or more of benzoyl peroxide, cumene hydroperoxide, tert-butyl hydroperoxide, 2, 4-dichlorobenzoyl peroxide and lauroyl peroxide.
7. The corrosion resistant composite armor layer material for neodymium iron boron according to claim 1, wherein said triisocyanate compound is one or more of 4,4',4 "-triphenylmethane triisocyanate, undecane-1, 6, 11-triyl triisocyanate, toluene-2, 4, 6-triyl triisocyanate.
8. The corrosion resistant composite armor material for neodymium iron boron according to claim 1, wherein said organotin catalyst is one or more of dibutyltin dilaurate, dibutyltin monomaleate, dibutyltin bis (isooctylmercaptoacetate).
9. The corrosion-resistant composite protective layer material for neodymium iron boron according to claim 1, wherein the film thickness of the base layer is 1-5 μm.
10. The corrosion-resistant composite protective layer material for neodymium iron boron according to claim 1, wherein the film thickness of the protective layer is 5 to 20 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111799052A (en) * | 2020-06-29 | 2020-10-20 | 浙江中杭新材料科技有限公司 | Sintered neodymium iron boron magnet with surface function rete |
| JP2022104855A (en) * | 2020-12-30 | 2022-07-12 | 包頭天和磁気材料科技股▲ふん▼有限公司 | Corrosion-resistant neodymium iron-boron magnet, surface treatment method, and usage of hydroxyl group compound |
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| JP7237108B2 (en) | 2020-12-30 | 2023-03-10 | 包頭天和磁気材料科技股▲ふん▼有限公司 | Corrosion resistant neodymium iron boron magnet, surface treatment method and use of hydroxyl compound |
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